Modular, mobile, and automated solvent extraction and distillation systems, and methods of using the same

ABSTRACT

Some variations provide an automated system for solvent extraction of a feed stock to produce a botanical extract, fats, oils, or other desirable solute, comprising: an extraction reactor; a distillation unit; and a second-stage purge chamber or a second-stage purge process utilizing the extraction reactor itself. The second-stage purge chamber or process receives or holds the solid material along with a heated inert non-condensable gas and/or solvent vapor, to recover residual solvent contained in the solid material. Other variations provide a process comprising: feeding a raw material and a solvent into an extraction reactor; generating dissolved material in rich solvent and extracted solid material; distilling the rich solvent to generate purified product and recovered solvent; conveying the solid material and a heated inert non-condensable gas and/or solvent vapor into a second-stage purge chamber, or holding the solid material in the same vessel, to recover residual solvent; and recovering the purified product.

PRIORITY DATA

This patent application is a non-provisional application claimingpriority to U.S. Provisional Patent App. No. 62/607,381, filed on Dec.19, 2017, which is hereby incorporated by reference herein.

FIELD OF THE INVENTION

The present invention generally relates to solvent-based extractionsystems and methods for extracting botanicals, other compositions ofmaterials containing desirable solutes, from plant materials, biomass,or other desirable feed stock.

BACKGROUND OF THE INVENTION

A botanical extract is an herbal or product ingredient with desirableflavor, aroma, or nutritive quality that is removed from the tissue of aplant, usually by treating it with a solvent, to be used for aparticular purpose. Botanical extracts have been used as a source ofmedicine throughout history and continue to serve as the basis for manypharmaceuticals, cosmeceuticals, and nutraceuticals today.

Solvent extractions of essential oils have occurred for centuries. Mostearly applications employed the use of commonly available oils likeolive oil and vegetable oils, based on direct contact of the oil withthe plant material or seeds of the desired essential oil. These wereused in early medicine, food enhancements, and preservatives. Thisprocess was very inefficient and only a minor portion of the plant'scompounds were transferred to the oil carrier. Steam stripping was laterused and proved to be far more efficient. Steam extractions are widelyused today. However, the high temperatures of the steam stripping cyclewill damage some of the targeted compounds.

The phytochemical composition of many plants has changed over time, withdomestication of agricultural crops resulting in enhanced content ofsome bioactive compounds and diminished content of others. Plantscontinue to serve as a valuable source of therapeutic compounds becauseof their vast biosynthetic capacity. Due to modern breakthroughs inscience, technology, and engineering, global markets are just nowadopting and have a deeper awareness of the medicinal, therapeutic, andalternative-energy applications, to name a few uses of botanicalextracts. Valuable botanical extracts include chamomile, dandelion,echinacea, marigold, lavender, cannabis, hemp, and many othertherapeutic plants and herbs that organically grow in our ecosystem.

The problem that currently exists in botanical extraction processing isthat typical manufacturing methods are limited in capacity, capability,and consistency. Present systems are generally small, single-batch,mixed-phase solvent systems designed and operated for small throughputs.Existing customer pains include slow processing times, inconsistentoutput quality and yield, low volume capability, high cost, andlogistical expense. The increased demand in processing capabilities forbotanical extractions is proving that existing technologies are not onlyincapable of handling the volume but they are also unsustainableprocessing solutions.

Prior art would have the operator manually fill the extraction vessel,rinse the plant material, and then wait to remove excess solvent viaevaporation, pressure to squeeze the residual retained in the biomass,spinning, or other mechanical processes to remove the remaining solvent.Then the operator manually removes content from the extraction vessel,exposing the operator to risk of contact with residual solvent beingexposed to environment, at the same time losing valuable high-qualitylaboratory or food-grade solvents. Then the operator manually refills itto repeat the action.

Because the market dependency and growth for botanical extraction israpidly expanding, there is an immediate need for larger-scale solutionsof high efficiency processing. In view of the prior art, problemsinclude material handling, distillation time, recovery of solvent, andremoval of the extract from the machine. There is a desire for removalof target compounds from plant materials without damage to thecompounds, and at high yields.

SUMMARY OF THE INVENTION

The present invention addresses the aforementioned needs in the art, aswill now be summarized and then further described in detail below.

Some variations provide an automated system for solvent extraction of aplant-based raw material or other feed stock biomass material to producea botanical extract, fats, oils, or other desirable solute, the systemcomprising:

(a) an extraction reactor configured with (i) a sealed feed inlet forfeeding a plant-based solid raw material or other type of desired inputmaterial, (ii) a solvent inlet for introducing lean solvent to theextraction reactor, (iii) one or more gas ports for introducing solventvapor and/or an inert non-condensable gas to the extraction reactorand/or for removing gases from the extraction reactor, (iv) optionally,a refrigeration cycle with the interior of the extraction vessel actingas an evaporator of the solvent, to sub-cool the substrate feed stockprior to extracting; (v) a solid outlet for conveying solid material outof the extraction reactor; and (vi) a product outlet for removing richsolvent containing a botanical or other variety of extract out of theextraction reactor;

(b) a closed-loop continuous-flow distillation unit configured togenerate purified botanical extract and recovered solvent, andpotentially valuable co-product fractions; and

(c) optionally a second-stage purge chamber configured to (i) receivethe solid material and (ii) receive a heated inert non-condensable gasand/or a solvent vapor, wherein the second-stage purge chamber iseffective to recover residual solvent contained in the solid material.

In some embodiments, the solvent is selected from the group consistingof but not limited to ethanol, isopropyl alcohol, methanol, pentane,dimethyl ether, chlorofluorocarbons, acetone, hexane, n-butane,isobutane, n-propane, isomers thereof, and combinations of any of theforegoing. In certain embodiments, the solvent is n-butane or n-propane.

In some embodiments, the inert non-condensable gas is selected from thegroup consisting of nitrogen, carbon dioxide, argon, helium, andcombinations thereof. In certain embodiments, the inert non-condensablegas is nitrogen.

The second-stage purge chamber is preferably present in embodiments inwhich the material is not dried within the initial extraction chamber.The second-stage purge chamber may be in communication with a heatexchanger to heat the residual solvent and/or the solvent vapor. Thesecond-stage purge chamber may be in communication with a heat-jacketedspool, pipe, or vessel containing an auger to agitate the solidmaterial. The second-stage purge chamber may be in communication with acondenser to condense the residual solvent for recovery.

In some embodiments, the system further comprises a liquid manifold thatis in flow communication with the solvent inlet, the product outlet, orboth of the solvent inlet and the product outlet.

In some embodiments, the system further comprises a gas manifold that isin flow communication with the one or more gas ports, the second-stagepurge chamber, or both of the one or more gas ports and the second-stagepurge chamber.

In some embodiments, the system further comprises a vacuum manifold thatis in flow communication with the one or more gas ports, thesecond-stage purge chamber, or both of the one or more gas ports and thesecond-stage purge chamber.

In some embodiments, the system further comprises a recovery manifoldthat is in flow communication with the extraction reactor, thedistillation unit, the second-stage purge chamber, or any combinationthereof.

The system is preferably capable of operating from full vacuum to about350 psig. However, the system is not limited to operation in thispressure range.

The system may be modular and may be arranged in a single extractiontrain or in multiple extraction trains. Also, the system is preferablyportable.

Other variations of the invention provide a process for producing abotanical extract, fats, oils, or other desirable solute from aplant-based raw material, biomass, or other feed stock material, theprocess comprising:

(a) feeding a plant-based solid raw material or other type of desiredinput material (e.g., biomass material) into an extraction reactor;

(b) introducing a lean solvent into the extraction reactor;

(c) introducing an inert, non-condensable gas into the extractionreactor;

(d) operating the extraction reactor under effective reaction conditionsto generate dissolved botanical extract, fats, oils, or other desirablesolute in rich solvent and solid material (that remains followingextraction of a portion into the liquid phase);

(e) distilling the rich solvent to generate purified botanical extract,fats, oils, or other desirable solute and recovered solvent;

(f) conveying the solid material and a heated inert non-condensable gasinto a second-stage purge chamber, operated to recover residual solventcontained in the solid material; and

(g) recovering the purified botanical extract, fats, oils, or otherdesirable solute.

In some embodiments, the plant-based solid raw material or other biomassmaterial is selected from the group consisting of whole plant,botanicals, plant seeds, plant components, and combinations thereof, orother materials not derived from plants.

The solvent may be selected from the group consisting of ethanol,isopropyl alcohol, methanol, pentane, dimethyl ether,chlorofluorocarbons, acetone, hexane, n-butane, isobutane, n-propane,isomers thereof, and combinations of any of the foregoing. The solventis typically in the liquid phase within the extraction reactor, but thesolvent may be at least partially in the vapor phase within theextraction reactor, depending on choice of solvent, extraction reactionconditions, and transient operations. The recovered residual solvent maybe recycled as at least a portion of the lean solvent in step (b).

The non-condensable gas may be selected from the group consisting ofnitrogen, carbon dioxide, argon, helium, and combinations thereof.

The effective reaction conditions for step (d) may include an extractiontemperature from about −80° C. to about 100° C., for example. Theeffective reaction conditions may include a pressure from full vacuum toabout 225 psig, for example. The effective reaction conditions mayinclude a solid-phase residence time from about 5 minutes to about 1hour, for example. In some embodiments, the effective reactionconditions include constant agitation within the extraction reactor,such as by an agitator auger, sonication, or both of these.

In certain embodiments, the process includes applying heating, cooling,pressure, and/or vacuum at a plurality of locations within the processto facilitate movement of the solvent between steps of the process.

In certain optional embodiments, the process includes using a solvent ina refrigeration cycle with the interior of the extraction vessel actingas an evaporator to sub-cool the substrate feed stock (i.e., theplant-based solid raw material or other type of desired input material)prior to extracting the substrate feed stock. The solvent for therefrigeration cycle may be the same solvent as the extraction solventintroduced in step (b), or may be an additional solvent.

Step (f) may be referred to as a “second-stage purge process.” In someembodiments, step (f) comprises conveying the solid material and theheated inert non-condensable gas and/or the solvent vapor into asecond-stage purge chamber, operated to recover the residual solventcontained in the solid material. In other embodiments, step (f)comprises holding the solid material within the extraction reactor,introducing the heated inert non-condensable gas and/or the solventvapor into the extraction reactor, and recovering the residual solventcontained in the solid material. A combination is also possible, whereinstep (f) includes both conveying the solid material and the heated inertnon-condensable gas and/or the solvent vapor into a second-stage purgechamber, as well as holding the solid material within the extractionreactor, and introducing the heated inert non-condensable gas and/or thesolvent vapor into both the second-stage purge chamber and theextraction reactor, and recovering residual solvent from both.

The process may be operated as a continuous or semi-continuous process.Preferably, the process is automated, at least in part.

In some embodiments, the extraction reactor is operated in adual/multi-parallel operation cycle. In other embodiments, theextraction reactor is operated in a dual/multi-cyclical operation cycle.

The purified botanical extract, fats, oils, or other desirable solutemay include one or more essential oils, for example. In someembodiments, the purified botanical extract, fats, oils, or otherdesirable solute is obtained in a product yield of at least about 15%(such as greater than 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%,or 20%) based on weight of the plant-based solid raw material or otherbiomass material.

The plant-based solid raw material or other biomass material may beprocessed at a rate of at least 1,000 lb/day, for example.

Optionally, the solid material recovered from step (f) may be furtherprocessed to generate nutraceutical, pharmaceutical, cosmeceutical,biofuel, or biochemical co-products.

Some variations provide a method of recovering solid material andresidual solvent obtained from an extraction reactor, the methodcomprising:

(a) obtaining a solid material from an extraction reactor, wherein thesolid material contains a residual solvent;

(b) subjecting the solid material and a heated inert non-condensable gasand/or a solvent vapor to a second-stage purge process (also referred toherein as a flash purge), operated to recover the residual solventcontained in the solid material; and

(c) recovering the solid material.

In some embodiments, the second-stage purge process comprises conveyingthe solid material and the heated inert non-condensable gas and/or thesolvent vapor into a second-stage purge chamber, operated to recover theresidual solvent contained in the solid material.

Alternatively, or additionally, in some embodiments the second-stagepurge process comprises holding the solid material within the extractionreactor, introducing the heated inert non-condensable gas and/or thesolvent vapor into the extraction reactor, and recovering the residualsolvent contained in the solid material.

The solid material recovered from step (c) may be used or furtherprocessed to generate nutraceutical, pharmaceutical, cosmeceutical,biofuel, or biochemical co-products.

Any of the disclosed processes or methods may utilize any of the systemsdisclosed herein, or portions thereof. The present invention alsoprovides a product produced by any of the processes described.

BRIEF DESCRIPTION OF THE DRAWING

FIG. 1 depicts a simplified block flow diagram of some system andprocess variations of the invention.

DETAILED DESCRIPTION OF EMBODIMENTS OF THE INVENTION

The materials, compositions, structures, systems, and methods of thepresent invention will be described in detail by reference to variousnon-limiting embodiments.

This description will enable one skilled in the art to make and use theinvention, and it describes several embodiments, adaptations,variations, alternatives, and uses of the invention. These and otherembodiments, features, and advantages of the present invention willbecome more apparent to those skilled in the art when taken withreference to the following detailed description of the invention inconjunction with the accompanying drawings.

As used in this specification and the appended claims, the singularforms “a,” “an,” and “the” include plural referents unless the contextclearly indicates otherwise. Unless defined otherwise, all technical andscientific terms used herein have the same meaning as is commonlyunderstood by one of ordinary skill in the art to which this inventionbelongs.

Unless otherwise indicated, all numbers expressing conditions,concentrations, dimensions, and so forth used in the specification andclaims are to be understood as being modified in all instances by theterm “about.” Accordingly, unless indicated to the contrary, thenumerical parameters set forth in the following specification andattached claims are approximations that may vary depending at least upona specific analytical technique.

The term “comprising,” which is synonymous with “including,”“containing,” or “characterized by” is inclusive or open-ended and doesnot exclude additional, unrecited elements or method steps. “Comprising”is a term of art used in claim language which means that the named claimelements are essential, but other claim elements may be added and stillform a construct within the scope of the claim.

As used herein, the phrase “consisting of” excludes any element, step,or ingredient not specified in the claim. When the phrase “consists of”(or variations thereof) appears in a clause of the body of a claim,rather than immediately following the preamble, it limits only theelement set forth in that clause; other elements are not excluded fromthe claim as a whole. As used herein, the phrase “consisting essentiallyof” limits the scope of a claim to the specified elements or methodsteps, plus those that do not materially affect the basis and novelcharacteristic(s) of the claimed subject matter.

With respect to the terms “comprising,” “consisting of” and “consistingessentially of” where one of these three terms is used herein, thepresently disclosed and claimed subject matter may include the use ofeither of the other two terms. Thus in some embodiments not otherwiseexplicitly recited, any instance of “comprising” may be replaced by“consisting of” or, alternatively, by “consisting essentially of.”

The present invention is premised on processes, systems, and methods forthe extraction and recovery of plant or other compounds (e.g., essentialoils), employing liquid-phase solvents that are recovered and reused ina continuous operation. In various embodiments, compositions containingdesirable solutes are removed from a material by utilizing a solventwith compatible polarities.

The raw material may be provided in the form of dried and cut wholeplant botanicals and seeds, for example. In this disclosure, “biomassmaterial” is intended to include any material composition that iscapable of providing, by the disclosed methods, botanical extract, fats,oils, or other desirable solute(s).

The finished product may be produced in the form of refined andunrefined oil, powder isolates and cakes, for example. In someembodiments, products include compounds found in algae or other biomass;compounds rich in oils, fats, and/or resins; or compounds that requirecontained environmental batching systems to provide safety to the useror allow for significant atmospheric phase-change controls.

In some variations, the present invention allows adjustable control ofthe physical contact and residence time of the extractions. The presentinvention allows continuous extractions of plant essences and oils whileproviding a liquid solvent extraction cycle. The residence time of theliquid solvent extraction cycle may be controlled within the system'ssequence control and can be varied to achieve the desired extractionefficiency for various plant matter being processed. The mechanicalconfiguration allows commercial-scale extractions of plant essences andoils with much higher efficiencies and throughputs than currenttechnologies. The system configuration allows the use of differentsolvents, allowing the system to be used on a variety of extractions.This will allow the system to be employed within a year-round harvestcycle, for a variety of markets.

Some embodiments utilize a large-scale botanical extraction system usinglow-pressure, high-yield organic solvents with modular capabilities forease of logistics. What is provided is industrial scale processing ofbotanical extraction, distillation, and fractionation. The botanicalextraction system is capable of processing at least 1,000 lb of rawmaterial per day, which is ten times current industry standard, withyields up to 20% of product, which is twice the current industrystandard. Mobilization provides unique flexibility previously notoffered for similar solutions. All process flow systems are preferablycomputer-automated. The mechanical configuration can be arranged andoperated with single or multiple extraction trains, each being deliveredfeed stock through a sealed feed charge hopper, for example. Theextraction train can be operated in a single process operations cycle, adual/multi-parallel process operations cycle, or a dual/multi-cyclicalprocess operations cycle. This allows for flexibility of run cycles andthroughput. Note that “dual/multi” refers to 2 or more, such as 3, 4, 5,or more.

One benefit associated with this invention is the reduction in delaysbetween extraction cycles, or batches with fully automated materialhandling through mechanical and computer-aided functions. In preferredembodiments, contact between the plant material and the solvent isenhanced via constant agitation, and solvent rinse and recovery cyclesare automated with electronic controls. These benefits ultimatelyincrease efficiency, improve recovery of solvent, and improve safety byremoving human error from the extraction and distillation process(especially while using volatile solvents). The system can operate up to24 hours per day, if desired.

These new advantages remove the delay between batch-distilling excesssolvent by creating the ability of adding additional chambers or“modules” while sharing the primary operating systems between multiplestages of operation. So while one module is performing the extraction byabsorbing soluble content retained in the plant parts, the other modulescan be finishing with their own extraction process and will be purgingthe residual plant material and any excess solvent contained within theextraction vessel preparing it for another run. Different solvents canalso be used depending on desirable features of solubility. Examplesinclude, but are not limited to, ethanol, isopropyl alcohol, methanol,pentane, dimethyl ether, chlorofluorocarbons, acetone, hexane, n-butane,isobutane, n-propane, or a mixture of two or more of these. In somepreferred embodiments, n-butane or n-propane is employed.

One of the significant components of the material handling is a shaftseal and motor mount assembly. In some embodiments, to meet the specificapplications of pressure and solvent, preferably an articulating seal isused, capable of withstanding full vacuum up to 350 psig of internalpressure along with intermittent solvent exposure. Note that the presentinvention is not limited to any particular pressure range.

Passive and active phase controls may increase the distillation processflow efficiency through engineered heating, cooling, and with pressurecontrol compressors. By applying heat, cooling, pressure, and/or avacuum at strategic points within the process, we can facilitate themovement of solvents between the various steps of the process, takingadvantage of specific physical properties of the solvents within thesedifferent conditions. This will allow shorter cycle times and allowcontrol over the parameters within the extraction cycle which canincrease or decrease solubility of certain desirable or undesirablecompounds.

Optionally, the process uses a solvent in a refrigeration cycle with theinterior of the extraction vessel acting as an evaporator to sub-coolthe substrate feed stock (i.e., the plant-based solid raw material orother type of desired input material) prior to extracting it. Thesolvent for the refrigeration cycle is typically the same solvent as theextraction solvent, but in principle the refrigeration solvent could bea different chemical introduced in addition to the extraction solvent.

A significant system feature is the second-stage purge chamber.Likewise, a significant process feature is the second-stage purgeprocess. Within the process, an inert, non-condensable gas such asnitrogen is heat cycled through a post-extraction process chamberdesigned with the intention of removing all residual solvent from thepreviously washed plant material in a closed loop. The second-stagepurge chamber is attached to a blower or compressor that forces theheated solvent vapor or non-condensable gas through a heated heatexchanger, then through a heat-jacketed spool containing a continualauger or mixer and designed to agitate the entire volume of remainingpreviously washed plant material against the heated surface whileblowing the hot vapor or non-condensable gas through the interior ofthis vessel—thus picking up any residual solvent and condensing it offfor a full recovery of residual solvent prior to ejecting the remainingbyproduct.

The system preferably will automatically monitor system status andrespond to desired process needs (pressure or temperature adjustment,physical process action, and response), through PLC automation of thecontrolled valves, pumps, heating and cooling systems, and monitoring ofall applicable process data, through instrumentation, for positivestatus confirmation. This includes automated hazard responses tounforeseen disastrous conditions, for safety of operator and property.The automation of the previously described steps will allow efficiencyimprovements with flexibility to upgrade the capabilities, volumes,pumping power, temperatures, and pressures as needed for a wide varietyof solvents, types and grades of botanical input material, and levels ofcontrol to refine the end product through precise temperature, pressure,and timing controls. This process records pertinent process datarecorded for each process to track with the production batches forstatistical tracking of end product quality and yield efficiency. Thiscan then be applied, into a flexible automation system, to adjustprocess parameters to ultimately have the optimal refinement parameterspreprogrammed as a “recipe” based on the applicable input material.

Preferred system and process configurations avoid the need to manuallyload and unload the machine itself. In preferred embodiments, there isautomation of each step and built-in safety protocols.

Some variations provide an automated system for solvent extraction of aplant-based raw material, biomass or other feed stock material toproduce a botanical extract, fats, oils, or other desirable solute, thesystem comprising:

(a) an extraction reactor configured with (i) a sealed feed inlet forfeeding a plant-based solid raw material or other type of desired inputmaterial, (ii) a solvent inlet for introducing lean solvent to theextraction reactor, (iii) one or more gas ports for introducing solventvapor and/or an inert non-condensable gas to the extraction reactorand/or for removing gases from the extraction reactor, (iv) optionally,a refrigeration cycle with the interior of the extraction vessel actingas an evaporator of the solvent, to sub-cool the substrate feed stockprior to extracting; (v) a solid outlet for conveying solid material outof the extraction reactor; and (vi) a product outlet for removing richsolvent containing a botanical or other variety of extract out of theextraction reactor;

(b) a closed-loop continuous-flow distillation unit configured togenerate purified botanical extract and recovered solvent, andpotentially valuable co-product fractions; and

(c) optionally a second-stage purge chamber configured to (i) receivethe solid material and (ii) receive a heated inert non-condensable gasand/or a solvent vapor, wherein the second-stage purge chamber iseffective to recover residual solvent contained in the solid material.

In some embodiments, the solvent is selected from the group consistingof but not limited to ethanol, isopropyl alcohol, methanol, pentane,dimethyl ether, chlorofluorocarbons, acetone, hexane, n-butane,isobutane, n-propane, isomers thereof, and combinations of any of theforegoing. In certain embodiments, the solvent is n-butane or n-propane.

In some embodiments, the inert non-condensable gas is selected from thegroup consisting of nitrogen, carbon dioxide, argon, helium, andcombinations thereof. In certain embodiments, the inert non-condensablegas is nitrogen.

The second-stage purge chamber is preferably present in embodiments inwhich the material is not dried within the initial extraction chamber.The second-stage purge chamber may be in communication with a heatexchanger to heat the residual solvent and/or the solvent vapor. Thesecond-stage purge chamber may be in communication with a heat-jacketedspool, pipe, or vessel containing an auger to agitate the solidmaterial. The second-stage purge chamber may be in communication with acondenser to condense the residual solvent for recovery.

In some embodiments, the system further comprises a liquid manifold thatis in flow communication with the solvent inlet, the product outlet, orboth of the solvent inlet and the product outlet.

In some embodiments, the system further comprises a gas manifold that isin flow communication with the one or more gas ports, the second-stagepurge chamber, or both of the one or more gas ports and the second-stagepurge chamber.

In some embodiments, the system further comprises a vacuum manifold thatis in flow communication with the one or more gas ports, thesecond-stage purge chamber, or both of the one or more gas ports and thesecond-stage purge chamber.

In some embodiments, the system further comprises a recovery manifoldthat is in flow communication with the extraction reactor, thedistillation unit, the second-stage purge chamber, or any combinationthereof.

The system is preferably capable of operating from full vacuum to about350 psig. However, the system is not limited to operation in thispressure range.

The system may be modular and may be arranged in a single extractiontrain or in multiple extraction trains. Also, the system is preferablyportable.

Other variations of the invention provide a process for producing abotanical extract, fats, oils, or other desirable solute from aplant-based raw material or other biomass material, the processcomprising:

(a) feeding a plant-based solid raw material or other biomass materialinto an extraction reactor;

(b) introducing a lean solvent into the extraction reactor;

(c) introducing an inert, non-condensable gas and/or a solvent vaporinto the extraction reactor;

(d) operating the extraction reactor under effective reaction conditionsto generate dissolved botanical extract, fats, oils, or other desirablesolute in rich solvent and solid material (that remains followingextraction of a portion into the liquid phase);

(e) distilling the rich solvent to generate purified botanical extract,fats, oils, or other desirable solute and recovered solvent;

(f) conveying the solid material and a heated inert non-condensable gasinto a second-stage purge chamber, operated to recover residual solventcontained in the solid material; and

(g) recovering the purified botanical extract, fats, oils, or otherdesirable solute.

In some embodiments, the plant-based solid raw material or other biomassmaterial is selected from the group consisting of whole plant,botanicals, plant seeds, plant components, and combinations thereof, orother materials not derived from plants.

The solvent may be selected from the group consisting of but not limitedto ethanol, isopropyl alcohol, methanol, pentane, dimethyl ether,chlorofluorocarbons, acetone, hexane, n-butane, isobutane, n-propane,isomers thereof, and combinations of any of the foregoing. The solventis typically in the liquid phase within the extraction reactor, but thesolvent may be at least partially in the vapor phase within theextraction reactor, depending on choice of solvent, extraction reactionconditions, and transient operations. The recovered residual solvent maybe recycled as at least a portion of the lean solvent in step (b).

The non-condensable gas may be selected from the group consisting ofnitrogen, carbon dioxide, argon, helium, and combinations thereof.

The effective reaction conditions for step (d) may include a temperaturefrom about −80° C. to about 100° C., for example. The effective reactionconditions include a pressure from full vacuum to about 225 psig, forexample. The effective reaction conditions include a solid-phaseresidence time from about 5 minutes to about 1 hour, for example. Insome embodiments, the effective reaction conditions include constantagitation within the extraction reactor, such as by an agitator auger,sonication, or both of these.

In certain embodiments, the process includes applying heating, cooling,pressure, and/or vacuum at a plurality of locations within the processto facilitate movement of the solvent between steps of the process.Optionally the solvent is utilized in a refrigeration cycle with theinterior of the extraction vessel acting as an evaporator to sub-coolthe substrate feed stock prior to extracting in step (d). Therefrigeration cycle may be conducted between steps (a) and (b), withinstep (b), between steps (b) and (c), within step (c), or between steps(c) and (d).

Step (f) may be referred to as a “second-stage purge process,” whetheror not there is physically a second-stage purge chamber, or whether ornot the extraction reactor itself is utilized for a flash purge.

In some embodiments, step (f) comprises conveying the solid material andthe heated inert non-condensable gas and/or the solvent vapor into asecond-stage purge chamber, operated to recover the residual solventcontained in the solid material. In other embodiments, step (f)comprises holding the solid material within the extraction reactor,introducing the heated inert non-condensable gas and/or the solventvapor into the extraction reactor, and recovering the residual solventcontained in the solid material. A combination is also possible, whereinstep (f) includes both conveying the solid material and the heated inertnon-condensable gas and/or the solvent vapor into a second-stage purgechamber, as well as holding the solid material within the extractionreactor, and introducing the heated inert non-condensable gas and/or thesolvent vapor into both the second-stage purge chamber and theextraction reactor, and recovering residual solvent from both.

The process may be operated as a continuous or semi-continuous process.Preferably, the process is automated, at least in part.

In some embodiments, the extraction reactor is operated in adual/multi-parallel operation cycle. In other embodiments, theextraction reactor is operated in a dual/multi-cyclical operation cycle.

The purified botanical extract, fats, oils, or other desirable solutemay include one or more essential oils, for example. In someembodiments, the purified botanical extract, fats, oils, or otherdesirable solute is obtained in a product yield of at least about 15%(such as greater than 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%,or 20%) based on weight of the plant-based solid raw material or otherbiomass material.

The plant-based solid raw material or other biomass material may beprocessed at a rate of at least 1,000 lb/day, for example.

Optionally, the solid material recovered from step (f) may be furtherprocessed to generate nutraceutical, pharmaceutical, cosmeceutical,biofuel, or biochemical co-products.

Some variations provide a method of recovering solid material andresidual solvent obtained from an extraction reactor, the methodcomprising:

(a) obtaining a solid material from an extraction reactor, wherein thesolid material contains a residual solvent (such as a solvent disclosedabove);

(b) subjecting the solid material and a heated inert non-condensable gas(such as a non-condensable gas disclosed above) and/or a solvent vapor(which may be the same solvent or a different solvent as the residualsolvent) to a second-stage purge process, operated to recover theresidual solvent contained in the solid material; and

(c) recovering the solid material.

The solid material may be obtained directly from an extraction reactordirectly, e.g. an adjacent extraction reactor at the same site. In otherembodiments, the extraction reactor is located elsewhere, and the solidmaterial (with residual solvent) is obtained and then processed usingthe above-described method.

The second-stage purge process is also referred to herein as a flashpurge. In some embodiments, the second-stage purge process comprisesconveying the solid material and the heated inert non-condensable gasand/or the solvent vapor into a second-stage purge chamber, operated torecover the residual solvent contained in the solid material.Alternatively, or additionally, in some embodiments the second-stagepurge process comprises holding the solid material within the extractionreactor, introducing the heated inert non-condensable gas and/or thesolvent vapor into the extraction reactor, and recovering the residualsolvent contained in the solid material.

FIG. 1 depicts a simplified block flow diagram of some system, process,and method variations of the invention. The reference to “manifolds” inthis drawing will now be further explained, with reference to somenon-limiting embodiments.

Some preferred system embodiments employ a four-manifold design. Thesefour manifolds connect to the applicable vessels as follows:

1. Liquid Manifold. All liquid and solvent connections are in thismanifold. Filters and screens are self-cleanable via designed filtrationcollection and redundancy, as well as automated responses which willcontain particulate to desired filters.

2. Pressurized Gas. From a recovery tank, the gas (e.g., N₂) providesthe system pressure which combines through gas recovery from anextraction and purge vessel, and separates in the recovery vessel fromthe solvent which is condensed into a liquid and settles into the bottomof the recovery vessel. Gas (such as nitrogen) is provided for processneeds from the gas manifold. Under gas pressure, preferably no solventwill be in vapor form. Mixed gas and solvent is recovered from variousvessels, and the non-condensable remains a gas in the storage tank, butthe solvent drops out to liquid. The gas manifold provides pressure toseveral vessels, during specific steps where being at a higher pressureis advantageous.

3. Recovery Manifold. This connects and draws down pressure viacompression pump from all contained vessels into the recovery tank. Thissystem is particularly unique as it integrates with the PLC and operatorinterface to utilize a perpetual recovery system that self-cools therecovery pump while not directly drawing down any vessel's pressure.This creates an “always-ready” recovery access, and automated prioritycontrol for the most important vessels. Given that all vessels areacting simultaneously on their specific process step, the automationwill ensure that all vessels are able to drop their pressure, via therecovery manifold, within the closed-loop system, to the desiredprogrammed pressure for their given step, without interfering with anyother vessel's process step. This always-ready recovery will allow forconsiderable adaptability to variations in process volumes, andexpansion into a multi-extraction production system as is the expandedapplication of this designed technology.

4. Vacuum Manifold. This connects during normal operation to theextraction and flash-purge (i.e., second-stage purge) systems, as theyare the two systems that actively expose themselves to externalenvironment for inputting, and ejecting, material. Through automationinterlocks and safety lockouts, this vacuum manifold is the gateway tothe material valve access, as it contains a valve with ambient air draw,used as the final pressure leveling after the full gas recovery. Thevacuum manifold then, once the vessel is resealed, fully vacuums anyambient oxygen and air to a full vacuum, before the vessel is broughtback into the closed-loop system. This ensures that no oxygen, moisture,or external gasses enter the closed loop system.

The extraction reactor is the only vessel to be directly connected toall four manifolds. Other vessels connect to what is pertinent for theirvarious functions.

The operation, instrumentation, and control of the system's core designis to be adaptable to a variety of solvent types, processed botanicals,and flexibility as efficiencies improve for a seamless operatorinterface with a continuously operating extraction system. This includesflexibility in self-cleaning of all screen and filtration systems, andredundant auto-purging filtration that will recognize as filters reachend of life and require changeout. The operator will have full access,after a safe purge, to access any filters directly for service, cleaningor replacement, without interrupting the cycle times of the overallsystem. Lastly, a preferred implementation of the 4-manifold systemacross all vessels allows for the further expansion of the modularplatform for multi-extraction closed-loop systems utilizing the commonfour manifolds for increased cost and complexity efficiencies. Thesystem is designed to be capable of being expanded into multipleextraction vessels simultaneously integrating with the rest of thedesigned recovery and refinement infrastructure for the extractedsolvent.

Applications include various essential oils extractions, small lot hopsextraction for microbreweries, and cannabinoid compounds from industrialhemp facilities. Other applications include, but are by no means limitedto, medical cannabis; hemp applications in food, fuel, paint,healthcare, beer and feed; and the more traditional botanical extractsas essential oils for cosmeceutical and wellness markets and powderisolates for nutraceutical and pharmaceutical markets.

In this detailed description, reference has been made to multipleembodiments and to the accompanying drawing(s) in which are shown by wayof illustration specific exemplary embodiments of the invention. Theseembodiments are described in sufficient detail to enable those skilledin the art to practice the invention, and it is to be understood thatmodifications to the various disclosed embodiments may be made by askilled artisan, technician, or engineer.

Any of the disclosed processes or methods may utilize any of the systemsdisclosed herein, or portions thereof. The present invention alsoprovides a product produced by any of the processes described.

Where methods and steps described above indicate certain eventsoccurring in certain order, those of ordinary skill in the art willrecognize that the ordering of certain steps may be modified and thatsuch modifications are in accordance with the variations of theinvention. Additionally, certain steps may be performed concurrently ina parallel process when possible, as well as performed sequentially.

All publications, patents, and patent applications cited in thisspecification are herein incorporated by reference in their entirety asif each publication, patent, or patent application were specifically andindividually put forth herein.

The embodiments, variations, and figures described above should providean indication of the utility and versatility of the present invention.Other embodiments that do not provide all of the features and advantagesset forth herein may also be utilized, without departing from the spiritand scope of the present invention. Such modifications and variationsare considered to be within the scope of the invention defined by theclaims.

What is claimed is:
 1. An automated system for solvent extraction of aplant-based raw material or other biomass material to produce abotanical extract, fats, oils, or other desirable solute, said systemcomprising: (a) an extraction reactor configured with (i) a sealed feedinlet for feeding a plant-based solid raw material, biomass, or otherfeed stock material, (ii) a solvent inlet for introducing lean solventto said extraction reactor, (iii) one or more gas ports for introducingsolvent vapor and/or an inert non-condensable gas to said extractionreactor and/or for removing gases from said extraction reactor; (iv)optionally, a refrigeration cycle with the interior of said extractionreactor acting as an evaporator of said solvent, to sub-cool saidplant-based solid raw material, biomass or other feed stock material;(v) a solid outlet for conveying solid material out of said extractionreactor; and (vi) a product outlet for removing rich solvent containinga botanical extract, or other precipitate, out of said extractionreactor; (b) a closed-loop continuous-flow distillation unit configuredto generate purified botanical extract and recovered solvent; and (c) asecond-stage purge chamber configured to (i) receive said solid materialand (ii) receive a heated inert non-condensable gas and/or said solventvapor, wherein said second-stage purge chamber is effective to recoverresidual solvent contained in said solid material.
 2. The system ofclaim 1, wherein said second-stage purge chamber is in communicationwith a heat exchanger to heat said residual solvent and/or said solventvapor.
 3. The system of claim 1, wherein said second-stage purge chamberis in communication with a heat-jacketed spool, pipe, or vesselcontaining an auger to agitate said solid material.
 4. The system ofclaim 1, wherein said second-stage purge chamber is in communicationwith a condenser to condense said residual solvent for recovery.
 5. Thesystem of claim 1, wherein said system further comprises a liquidmanifold that is in flow communication with said solvent inlet, saidproduct outlet, or both of said solvent inlet and said product outlet.6. The system of claim 1, wherein said system further comprises a gasmanifold that is in flow communication with said one or more gas ports,said second-stage purge chamber, or both of said one or more gas portsand said second-stage purge chamber.
 7. The system of claim 1, whereinsaid system further comprises a vacuum manifold that is in flowcommunication with said one or more gas ports, said second-stage purgechamber, or both of said one or more gas ports and said second-stagepurge chamber.
 8. The system of claim 1, wherein said system furthercomprises a recovery manifold that is in flow communication with saidextraction reactor, said distillation unit, said second-stage purgechamber, or any combination thereof.
 9. The system of claim 1, whereinsaid system is modular.
 10. The system of claim 1, wherein said systemis portable.
 11. A process for producing a botanical extract, fats,oils, or other desirable solute from a plant-based raw material, biomassmaterial, or other desired feed stock, said process comprising: (a)feeding a plant-based raw material, biomass material, or other desiredfeed stock into an extraction reactor; (b) introducing a lean solventinto said extraction reactor; (c) introducing an inert non-condensablegas and/or a solvent vapor into said extraction reactor; (d) operatingsaid extraction reactor under effective reaction conditions to generate,in rich solvent, dissolved botanical extract, fats, oils, or otherdesirable solute, and solid material; (e) distilling said rich solventto generate purified botanical extract, fats, oils, or other desirablesolute, and recovered solvent; (f) exposing said solid material to aheated inert non-condensable gas and/or said solvent vapor, to recoverresidual solvent contained in said solid material; and (g) recoveringsaid purified botanical extract, fats, oils, or other desirable solute.12. The process of claim 11, wherein said plant-based raw material,biomass material, or other desired feed stock is selected from the groupconsisting of whole plant, botanicals, plant seeds, plant components,and combinations thereof.
 13. The process of claim 11, wherein said leansolvent includes a solvent selected from the group consisting ofethanol, isopropyl alcohol, methanol, pentane, dimethyl ether,chlorofluorocarbons, acetone, hexane, n-butane, isobutane, n-propane,isomers thereof, and combinations of any of the foregoing.
 14. Theprocess of claim 11, wherein said non-condensable gas is selected fromthe group consisting of nitrogen, carbon dioxide, argon, helium, andcombinations thereof.
 15. The process of claim 11, wherein saideffective reaction conditions include a temperature from about −80° C.to about 100° C., a pressure from full vacuum to about 350 psig, asolid-phase residence time from about 5 minutes to about 1 hour, andconstant agitation within said extraction reactor.
 16. The process ofclaim 11, wherein said process further comprises using said solvent in arefrigeration cycle with the interior of said extraction reactor actingas an evaporator to sub-cool said plant-based raw material, biomassmaterial, or other desired feed stock prior to step (d).
 17. The processof claim 11, wherein step (f) comprises conveying said solid materialand said heated inert non-condensable gas and/or said solvent vapor intoa second-stage purge chamber, operated to recover said residual solventcontained in said solid material.
 18. The process of claim 11, whereinstep (f) comprises holding said solid material within said extractionreactor, introducing said heated inert non-condensable gas and/or saidsolvent vapor into said extraction reactor, and recovering said residualsolvent contained in said solid material.
 19. The process of claim 11,wherein said recovered residual solvent is recycled as at least aportion of said lean solvent in step (b).
 20. The process of claim 11,wherein said purified botanical extract, fats, oils, or other desirablesolute is obtained in a product yield of at least about 15% based onweight of said plant-based solid raw material or other biomass material.21. The process of claim 11, wherein said process is continuous orsemi-continuous, and wherein said process is automated.
 22. A method ofrecovering solid material and residual solvent obtained from anextraction reactor, said method comprising: (a) obtaining a solidmaterial from an extraction reactor, wherein said solid materialcontains a residual solvent; (b) subjecting said solid material and aheated inert non-condensable gas and/or a solvent vapor to asecond-stage purge process, operated to recover said residual solventcontained in said solid material; and (c) recovering said solidmaterial.
 23. The method of claim 22, wherein said second-stage purgeprocess comprises conveying said solid material and said heated inertnon-condensable gas and/or said solvent vapor into a second-stage purgechamber, operated to recover said residual solvent contained in saidsolid material.
 24. The method of claim 22, wherein said second-stagepurge process comprises holding said solid material within saidextraction reactor, introducing said heated inert non-condensable gasand/or said solvent vapor into said extraction reactor, and recoveringsaid residual solvent contained in said solid material.